CN115650707A - Preparation method of magnesia-alumina transparent ceramic - Google Patents
Preparation method of magnesia-alumina transparent ceramic Download PDFInfo
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- CN115650707A CN115650707A CN202211374324.2A CN202211374324A CN115650707A CN 115650707 A CN115650707 A CN 115650707A CN 202211374324 A CN202211374324 A CN 202211374324A CN 115650707 A CN115650707 A CN 115650707A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 64
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical class [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 47
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000003756 stirring Methods 0.000 claims abstract description 46
- 239000006185 dispersion Substances 0.000 claims abstract description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920001661 Chitosan Polymers 0.000 claims abstract description 34
- 239000002804 dopamine agent Substances 0.000 claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- RGDDVTHQUAQTIE-UHFFFAOYSA-N 2-pentadecylphenol Chemical compound CCCCCCCCCCCCCCCC1=CC=CC=C1O RGDDVTHQUAQTIE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 77
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- -1 compound lanthanum oxide Chemical class 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 22
- 230000006872 improvement Effects 0.000 claims description 20
- GSWGDDYIUCWADU-UHFFFAOYSA-N aluminum magnesium oxygen(2-) Chemical compound [O--].[Mg++].[Al+3] GSWGDDYIUCWADU-UHFFFAOYSA-N 0.000 claims description 17
- 239000002041 carbon nanotube Substances 0.000 claims description 17
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 17
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 16
- 235000010413 sodium alginate Nutrition 0.000 claims description 16
- 229940005550 sodium alginate Drugs 0.000 claims description 16
- 239000000661 sodium alginate Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- ZSKXYSCQDWAUCM-UHFFFAOYSA-N 1-(chloromethyl)-2-dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1CCl ZSKXYSCQDWAUCM-UHFFFAOYSA-N 0.000 claims description 9
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 9
- 239000007983 Tris buffer Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000002715 modification method Methods 0.000 claims description 8
- 239000002048 multi walled nanotube Substances 0.000 claims description 8
- 229960005489 paracetamol Drugs 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 3
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims 2
- 229960003638 dopamine Drugs 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 2
- 239000000395 magnesium oxide Substances 0.000 abstract description 2
- 230000035699 permeability Effects 0.000 abstract description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- 150000002910 rare earth metals Chemical class 0.000 abstract description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 239000007822 coupling agent Substances 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 5
- 230000002195 synergetic effect Effects 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- LTPBRCUWZOMYOC-UHFFFAOYSA-N Beryllium oxide Chemical compound O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011885 synergistic combination Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to the technical field of transparent ceramics, and particularly discloses a preparation method of magnesia-alumina transparent ceramics, which comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 5 to 10 times of the total weight of the alumina according to the weight ratio of (8 to 12) to 1, then adding modified hydroxyapatite which is 2 to 5 percent of the total weight of the alumina, and stirring and mixing. According to the invention, aluminum oxide and magnesium oxide are used as matrixes for matching, graphene agent which is formed by matching graphene with hydrochloric acid solution, pentadecyl phenol and dopamine agent is adopted, and chitosan compounded lanthanum oxide solution is used as a rare earth active agent through lanthanum oxide, and the permeability of the product is improved through the assistance of chitosan and sulfuric acid solution, and the interfacial property among raw materials of the product is optimized, so that the strength and light transmittance effect of the product are enhanced in a coordinated manner.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a preparation method of magnesia-alumina transparent ceramics.
Background
Generally ceramics are opaque, but optical ceramics are transparent like glass, and are called transparent ceramics. The reason why the ceramic is generally opaque is that impurities and pores exist in the ceramic, the former absorbs light, and the latter scatters light, so that the ceramic is opaque. Therefore, if high-purity raw materials are selected and the pores are eliminated by the process, it is possible to obtain transparent ceramics. In the early days, transparent alumina ceramics were obtained by this method, and subsequently, many oxide series transparent ceramics such as sintered white corundum, magnesia, beryllia, yttria-zirconia, etc. were developed. Non-oxide transparent ceramics such as gallium arsenide, zinc sulfide, zinc selenide, magnesium fluoride, calcium fluoride, etc. have been developed recently.
The prior transparent ceramics have poor light transmittance and poor strength performance, and the coordination and improvement of the two performances are difficult points of the invention, on the basis of which the invention further improves and processes the transparent ceramics.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of magnesia-alumina transparent ceramics, so as to solve the problems in the background technology.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a preparation method of magnesium aluminum oxide transparent ceramic, which comprises the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 5 to 10 times of the total weight of the alumina according to the weight ratio of (8 to 12) to 1, then adding modified hydroxyapatite which is 2 to 5 percent of the total weight of the alumina, and stirring and mixing;
step two: washing and drying the product obtained in the step one, and sending the product into a ball mill for ball milling by 200-
300 meshes;
step three: placing the ball-milled product in the step two in a chitosan compound lanthanum oxide solution with the total amount of the ball-milled product being 3-5 times of the total amount of the ball-milled product, continuing ultrasonic dispersion treatment, finishing ultrasonic treatment, washing and drying;
step four: then the mixture is sent into a mould for static pressure treatment, the treatment pressure is 10-20MPa, and the treatment lasts for 1-2h;
step five: finally sintering at 1050-1150 ℃ for 10-20min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
Preferably, the preparation method of the dispersion regulator comprises the following steps:
s01: placing graphene in a hydrochloric acid solution which is 3-5 times of the total weight of the graphene, then adding pentadecyl phenol accounting for 5-10% of the total weight of the graphene and dopamine agent accounting for 1-5% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 1-3 parts by weight of hexadecyl trimethyl ammonium bromide into 5-10 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into the product S01, and stirring and mixing fully to obtain the dispersion regulator.
Preferably, the mass fraction of the hydrochloric acid solution is 5-10%.
Preferably, the dopamine agent is prepared by dispersing carbon nanotubes into a Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
The inventor of the invention finds that the strength performance and the light transmittance of the product are obviously reduced without adding modified hydroxyapatite, the performance of the product is deteriorated without adopting dispersion regulator treatment and chitosan compound lanthanum oxide solution treatment, dopamine agent is not added in the preparation of the dispersion regulator, graphene is not added in the preparation of the dispersion regulator, and the performance of the product is in a deterioration trend, so that the strength performance and the light transmittance of the product are excellent and the performance can be harmoniously improved only by adopting the dispersion regulator prepared by the method;
preferably, the mass fraction of the sodium alginate solution is 10-20%.
Preferably, the carbon nanotubes are multi-walled carbon nanotubes with a particle size of 10-20nm.
Preferably, the modification method of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into ethanol solvent 5-10 times of the total weight of hydroxyapatite, adding silane coupling agent 2-5% of the total weight of hydroxyapatite and paracetamol 1-3%, stirring thoroughly, washing with water, and drying to obtain modified hydroxyapatite.
Preferably, the silane coupling agent is a coupling agent KH560.
Preferably, the chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 4-8 parts of chitosan, 1-3 parts of lanthanum oxide and 20-30 parts of 45-55% sulfuric acid solution by mass fraction.
The inventor finds that the performance of the product tends to be deteriorated without adopting the treatment of a dispersion regulator and the treatment of a chitosan compound lanthanum oxide solution, and the hydroxyapatite can be modified by the synergistic combination of the treatment of the dispersion regulator and the treatment of the chitosan compound lanthanum oxide solution, so that the synergistic effect can be generated, and the performance improvement effect of the product can be enhanced.
Preferably, the operation steps of the heating temperature improvement treatment are as follows: heating to 1300-1320 deg.C at 1-3 deg.C/s, maintaining for 5-10min, and cooling to room temperature with 3-5 deg.C water.
Compared with the prior art, the invention has the following beneficial effects:
the magnesium aluminum oxide transparent ceramic is prepared by matching aluminum oxide and magnesium aluminum oxide serving as substrates, adopting graphene matched with a hydrochloric acid solution, pentadecyl phenol and a dopamine agent, simultaneously using raw materials such as cetyl trimethyl ammonium bromide and 4-aminophenylboronic acid for assistance, improving and optimizing the aluminum oxide and the magnesium aluminum oxide, adding flaky graphene serving as a substrate, performing dispersion assistance improvement on the dopamine agent prepared by carbon nano tubes, assisting and enhancing the strength and the light transmittance of the product substrate, adding modified hydroxyapatite with an auxiliary synergistic effect, enhancing the strength and the light transmittance of a product, using lanthanum oxide as a rare earth active agent in a chitosan-lanthanum oxide compounded solution, improving the permeability of the product by assisting the chitosan and a sulfuric acid solution, optimizing the interfacial property among the raw materials of the product, and further enhancing the strength and the light transmittance effect of the product in a coordinated manner.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the magnesium aluminum oxide transparent ceramic comprises the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 5 to 10 times of the total weight of the alumina according to the weight ratio of (8 to 12) to 1, then adding modified hydroxyapatite which is 2 to 5 percent of the total weight of the alumina, and stirring and mixing;
step two: washing and drying the product in the step one, and sending the product into a ball mill for ball milling by 200-
300 meshes;
step three: putting the ball-milled product in the step two into a chitosan compound lanthanum oxide solution with the volume 3-5 times of that of the ball-milled product, continuing ultrasonic dispersion treatment, wherein the ultrasonic power is 350-450W, the ultrasonic time is 10-20min, finishing ultrasonic treatment, washing with water, and drying;
step four: then the mixture is sent into a mould for static pressure treatment, the treatment pressure is 10-20MPa, and the treatment lasts for 1-2h;
step five: finally, sintering at 1050-1150 ℃ for 10-20min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
The preparation method of the dispersion regulator in this example is as follows:
s01: placing graphene in a hydrochloric acid solution which is 3-5 times of the total weight of the graphene, then adding pentadecyl phenol accounting for 5-10% of the total weight of the graphene and dopamine agent accounting for 1-5% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 1-3 parts by weight of hexadecyl trimethyl ammonium bromide into 5-10 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into the product S01, and stirring and mixing fully to obtain the dispersion regulator.
The mass fraction of the hydrochloric acid solution in this example is 5-10%.
The dopamine agent of the embodiment is prepared by dispersing carbon nanotubes into Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
The mass fraction of the sodium alginate solution in the embodiment is 10-20%.
The carbon nanotubes of this example are multiwalled carbon nanotubes with a particle size of 10-20nm.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps: adding hydroxyapatite into ethanol solvent 5-10 times of the total weight of hydroxyapatite, adding silane coupling agent 2-5% of the total weight of hydroxyapatite and paracetamol 1-3%, stirring thoroughly, washing with water, and drying to obtain modified hydroxyapatite.
The silane coupling agent of the present example is a coupling agent KH560.
The chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 4-8 parts of chitosan, 1-3 parts of lanthanum oxide and 20-30 parts of 45-55% sulfuric acid solution by mass fraction.
The operation steps of the temperature-raising heat improvement treatment of the embodiment are as follows: heating to 1300-1320 deg.C at 1-3 deg.C/s, maintaining for 5-10min, and cooling to room temperature with 3-5 deg.C water.
Example 1.
The preparation method of the magnesium aluminum oxide transparent ceramic comprises the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 5 times of the total amount of the alumina according to the weight ratio of 8 to 1, then adding modified hydroxyapatite accounting for 2 percent of the total amount of the alumina, and stirring and mixing;
step two: washing and drying the product obtained in the step one, and sending the product into a ball mill to ball-mill the product through a 200-mesh sieve;
step three: placing the ball-milled product in the step two into a chitosan compound lanthanum oxide solution with the total amount of the ball-milled product being 3 times that of the ball-milled product, continuing ultrasonic dispersion treatment, finishing ultrasonic treatment, washing with water and drying;
step four: then sending the mixture into a die for static pressure treatment, wherein the treatment pressure is 10MPa, and treating for 1h;
step five: finally, sintering at 1050 ℃ for 10min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
The preparation method of the dispersion regulator in this example is as follows:
s01: placing graphene in a hydrochloric acid solution which is 3 times of the total weight of the graphene, then adding pentadecylphenol accounting for 5% of the total weight of the graphene and dopamine agent accounting for 1% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 1 part by weight of hexadecyl trimethyl ammonium bromide into 5 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into the product S01, and stirring and mixing fully to obtain the dispersion regulator.
The mass fraction of the hydrochloric acid solution in this example was 5%.
The dopamine agent of the embodiment is prepared by dispersing carbon nanotubes into Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
The mass fraction of the sodium alginate solution in this example was 10%.
The carbon nanotubes of this example are multiwalled carbon nanotubes with a particle size of 10nm.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps: adding hydroxyapatite into an ethanol solvent which is 5 times of the total weight of the hydroxyapatite, then adding a silane coupling agent accounting for 2 percent of the total weight of the hydroxyapatite and paracetamol accounting for 1 percent of the total weight of the hydroxyapatite, fully stirring, and finally washing and drying to obtain the modified hydroxyapatite.
The silane coupling agent of the present example is a coupling agent KH560.
The chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 4 parts of chitosan, 1 part of lanthanum oxide and 20 parts of sulfuric acid solution with the mass fraction of 45%.
The operation steps of the temperature-raising heat improvement treatment of the embodiment are as follows: heating to 1300 deg.C at a rate of 1 deg.C/s, maintaining for 5min, and cooling with water at 3 deg.C to room temperature.
Example 2.
The preparation method of the magnesium aluminum oxide transparent ceramic comprises the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 10 times of the total amount of the alumina according to the weight ratio of 12 to 1, then adding modified hydroxyapatite which is 5 percent of the total amount of the alumina, and stirring and mixing;
step two: washing and drying the product obtained in the step one, and sending the product into a ball mill to be ball-milled for 300 meshes;
step three: placing the ball-milled product in the step two into a chitosan compound lanthanum oxide solution with the total amount of the ball-milled product being 3-5 times that of the ball-milled product, continuing ultrasonic dispersion treatment, and after the ultrasonic treatment, washing and drying;
step four: then the mixture is sent into a mould for static pressure treatment, the treatment pressure is 20MPa, and the treatment lasts for 2 hours;
step five: finally, sintering at 1150 ℃ for 20min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
The preparation method of the dispersion regulator in this example is as follows:
s01: placing graphene in a hydrochloric acid solution which is 5 times of the total weight of the graphene, then adding pentadecyl phenol accounting for 10% of the total weight of the graphene and dopamine agent accounting for 5% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 3 parts by weight of hexadecyl trimethyl ammonium bromide into 10 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into the product S01, and stirring and mixing fully to obtain the dispersion regulator.
The mass fraction of the hydrochloric acid solution in this example was 10%.
The dopamine agent in the embodiment is prepared by dispersing carbon nanotubes into a Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
The mass fraction of the sodium alginate solution in this example was 20%.
The carbon nanotubes of this example are multiwalled carbon nanotubes with a particle size of 20nm.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps: adding hydroxyapatite into an ethanol solvent which is 10 times of the total weight of the hydroxyapatite, then adding a silane coupling agent which is 5 percent of the total weight of the hydroxyapatite and paracetamol which is 3 percent of the total weight of the hydroxyapatite, fully stirring, and finally washing and drying to obtain the modified hydroxyapatite.
The silane coupling agent of the present example is a coupling agent KH560.
The chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 8 parts of chitosan, 3 parts of lanthanum oxide and 30 parts of sulfuric acid solution with mass fraction of 55%.
The operation steps of the temperature-raising heat improvement treatment of the embodiment are as follows: heating to 1320 deg.C at 3 deg.C/s, keeping the temperature for 10min, and cooling to room temperature with 5 deg.C water.
Example 3.
The preparation method of the magnesium aluminum oxide transparent ceramic comprises the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 7.5 times of the total amount of the alumina according to a weight ratio of 10;
step two: washing and drying the product obtained in the step one, and sending the product into a ball mill for ball milling to pass through a 250-mesh sieve;
step three: placing the ball-milled product in the step two into a chitosan compound lanthanum oxide solution with the total amount of the ball-milled product being 4 times that of the ball-milled product, continuing ultrasonic dispersion treatment, finishing ultrasonic treatment, washing with water and drying;
step four: then the mixture is sent into a mould for static pressure treatment, the treatment pressure is 15MPa, and the treatment time is 1.5h;
step five: and finally sintering at 1100 ℃ for 15min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
The preparation method of the dispersion regulator in this example is as follows:
s01: placing graphene in a hydrochloric acid solution with the weight 4 times of the total weight of the graphene, then adding pentadecyl phenol accounting for 7.5% of the total weight of the graphene and dopamine agent accounting for 3% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 2 parts by weight of hexadecyl trimethyl ammonium bromide into 5-10 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into S01, and stirring and mixing fully to obtain the dispersion regulator.
The mass fraction of the hydrochloric acid solution in this example was 7.5%.
The dopamine agent in the embodiment is prepared by dispersing carbon nanotubes into a Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
The mass fraction of the sodium alginate solution in this example was 15%.
The carbon nanotubes of this example are multiwalled carbon nanotubes with a particle size of 15nm.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps: adding hydroxyapatite into an ethanol solvent which is 7.5 times of the total weight of the hydroxyapatite, then adding a silane coupling agent which is 3.5 percent of the total weight of the hydroxyapatite and paracetamol which is 2 percent of the total weight of the hydroxyapatite, fully stirring, finally washing and drying to obtain the modified hydroxyapatite.
The silane coupling agent of the present example is a coupling agent KH560.
The chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 6 parts of chitosan, 2 parts of lanthanum oxide and 25 parts of sulfuric acid solution with the mass fraction of 50%.
The operation steps of the temperature-raising heat improvement treatment of the embodiment are as follows: heating to 1310 ℃ at the speed of 2 ℃/s, preserving heat for 7.5min, and finally cooling to room temperature by water at the temperature of 4 ℃.
Example 4.
The preparation method of the magnesium aluminum oxide transparent ceramic of the embodiment comprises the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 6 times of the total amount of the alumina according to a weight ratio of 9;
step two: washing and drying the product obtained in the first step, and sending the product into a ball mill for ball milling through a 200-mesh sieve;
step three: placing the ball-milled product in the step two in a chitosan compound lanthanum oxide solution with the total amount of the ball-milled product being 4 times that of the ball-milled product, continuing ultrasonic dispersion treatment, finishing ultrasonic treatment, washing with water and drying;
step four: then sending the mixture into a mould for static pressure treatment, wherein the treatment pressure is 12MPa, and treating for 1-2h;
step five: finally, sintering at 1060 ℃ for 12min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
The preparation method of the dispersion regulator in this example is as follows:
s01: placing graphene in a hydrochloric acid solution with the weight 4 times of the total weight of the graphene, then adding pentadecyl phenol accounting for 6% of the total weight of the graphene and dopamine agent accounting for 2% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 1.2 parts by weight of hexadecyl trimethyl ammonium bromide into 6 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into the product S01, and stirring and mixing fully to obtain the dispersion regulator.
The mass fraction of the hydrochloric acid solution in this example was 6%.
The dopamine agent in the embodiment is prepared by dispersing carbon nanotubes into a Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
The mass fraction of the sodium alginate solution in this example was 12%.
The carbon nanotubes of this example are multiwalled carbon nanotubes with a particle size of 15nm.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps: adding hydroxyapatite into an ethanol solvent 6 times of the total weight of the hydroxyapatite, then adding a silane coupling agent 3% of the total weight of the hydroxyapatite and paracetamol 1.2%, fully stirring, and finally washing and drying to obtain the modified hydroxyapatite.
The silane coupling agent of the present example is a coupling agent KH560.
The chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 5 parts of chitosan, 1.2 parts of lanthanum oxide and 2 parts of sulfuric acid solution with the mass fraction of 46%.
The operation steps of the temperature-raising heat improvement treatment of the embodiment are as follows: heating to 1310 ℃ at the speed of 1.2 ℃/s, preserving the heat for 6min, and finally cooling to room temperature by water at the temperature of 4 ℃.
Example 5.
The preparation method of the magnesium aluminum oxide transparent ceramic comprises the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 6 times of the total amount of the alumina according to a weight ratio of 9;
step two: washing and drying the product obtained in the step one, and sending the product into a ball mill for ball milling through a 220-mesh sieve;
step three: placing the ball-milled product in the step two in a chitosan compound lanthanum oxide solution with the total amount of the ball-milled product being 4 times that of the ball-milled product, continuing ultrasonic dispersion treatment, finishing ultrasonic treatment, washing with water and drying;
step four: then the mixture is sent into a mould for static pressure treatment, the treatment pressure is 18MPa, and the treatment time is 1.8h;
step five: and finally, sintering at 1130 ℃ for 18min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
The preparation method of the dispersion regulator in this example is as follows:
s01: placing graphene in a hydrochloric acid solution with the weight 4 times of the total weight of the graphene, then adding pentadecyl phenol accounting for 8% of the total weight of the graphene and dopamine agent accounting for 3% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 2 parts by weight of hexadecyl trimethyl ammonium bromide into 8 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into S01, and stirring and mixing fully to obtain the dispersion regulator.
The mass fraction of the hydrochloric acid solution in this example was 8%.
The dopamine agent of the embodiment is prepared by dispersing carbon nanotubes into Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
The mass fraction of the sodium alginate solution in this example was 18%.
The carbon nanotubes of this example are multiwalled carbon nanotubes with a particle size of 18nm.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps: adding hydroxyapatite into an ethanol solvent which is 8 times of the total weight of the hydroxyapatite, then adding a silane coupling agent accounting for 4 percent of the total weight of the hydroxyapatite and paracetamol accounting for 2 percent of the total weight of the hydroxyapatite, fully stirring, and finally washing and drying to obtain the modified hydroxyapatite.
The silane coupling agent of the present example is a coupling agent KH560.
The chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 6 parts of chitosan, 2 parts of lanthanum oxide and 28 parts of sulfuric acid solution with the mass fraction of 52%.
The operation steps of the temperature-raising heat improvement treatment of the embodiment are as follows: heating to 1315 ℃ at the speed of 2.8 ℃/s, keeping the temperature for 8min, and finally cooling to room temperature by water at the temperature of 4 ℃.
Comparative example 1.
In contrast to example 3, no modified hydroxyapatite was added.
Comparative example 2.
The difference from example 3 is that the modified hydroxyapatite is replaced by hydroxyapatite.
Comparative example 3.
In contrast to example 3, no dispersion regulator treatment was used.
Comparative example 4.
In contrast to example 3, no dopamine agent was added in the preparation of the dispersion modifier.
Comparative example 5.
The difference from example 3 is that no graphene was added in the preparation of the dispersion modifier.
Comparative example 6.
The difference from the example 3 is that the chitosan is not added to compound the lanthanum oxide solution.
The results of the performance measurements of examples 1 to 5 and comparative examples 1 to 6 are as follows
As can be seen from examples 1-5 and comparative examples 1-6, the product of example 3 of the present invention has excellent maximum transmittance of visible light and bending strength, and simultaneously the product of the present invention has excellent improvement effects on the maximum transmittance of visible light and bending strength compared with the comparative examples;
as can be seen from comparative examples 1-6, the strength performance and the light transmittance of the product are remarkably reduced without adding modified hydroxyapatite, the performance of the product is deteriorated without adopting dispersion regulator treatment and chitosan compound lanthanum oxide solution treatment, dopamine agent is not added in the preparation of the dispersion regulator, graphene is not added in the preparation of the dispersion regulator, and the performance of the product is in a deterioration trend, so that the strength performance and the light transmittance of the product are excellent and the performance can be harmoniously improved only by adopting the dispersion regulator prepared by the method;
in addition, the product is not treated by a dispersion regulator and treated by a chitosan compound lanthanum oxide solution, the performance of the product tends to be deteriorated, and the hydroxyapatite is modified by the synergistic effect of the dispersion regulator and the chitosan compound lanthanum oxide solution, so that the synergistic effect can be generated, and the performance improvement effect of the product is enhanced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to
The description is given according to the embodiments, but not every embodiment includes only one independent technical solution, and such description of the embodiments is only for the sake of clarity, and those skilled in the art should take the description as a whole, and the technical solutions in the embodiments may be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims (10)
1. The preparation method of the magnesia-alumina transparent ceramic is characterized by comprising the following steps:
the method comprises the following steps: adding alumina and magnesia-alumina into a dispersion regulator which is 5 to 10 times of the total weight of the alumina according to the weight ratio of (8 to 12) to 1, then adding modified hydroxyapatite which is 2 to 5 percent of the total weight of the alumina, and stirring and mixing;
step two: washing and drying the product obtained in the step one, and sending the product into a ball mill to ball-mill the product through 200-300 meshes;
step three: placing the ball-milled product in the step two into a chitosan compound lanthanum oxide solution with the total amount of the ball-milled product being 3-5 times that of the ball-milled product, continuing ultrasonic dispersion treatment, and after the ultrasonic treatment, washing and drying;
step four: then the mixture is sent into a mould for static pressure treatment, the treatment pressure is 10-20MPa, and the treatment lasts for 1-2h;
step five: finally, sintering at 1050-1150 ℃ for 10-20min, and then heating for thermal improvement treatment to obtain the magnesia-alumina transparent ceramic.
2. The method for preparing the magnesia-alumina transparent ceramic according to claim 1, wherein the dispersion modifier is prepared by the following steps:
s01: placing graphene in a hydrochloric acid solution which is 3-5 times of the total weight of the graphene, then adding pentadecylphenol accounting for 5-10% of the total weight of the graphene and dopamine accounting for 1-5% of the total weight of the graphene, and uniformly stirring to obtain a graphene agent;
s02: adding 1-3 parts by weight of hexadecyl trimethyl ammonium bromide into 5-10 parts by weight of sodium alginate solution, uniformly stirring, finally adding 4-aminophenylboronic acid, and fully stirring;
s03: and adding the product S02 into the product S01, and stirring and mixing fully to obtain the dispersion regulator.
3. The method for preparing the magnesium aluminum oxide transparent ceramic according to claim 2, wherein the mass fraction of the hydrochloric acid solution is 5-10%.
4. The method for preparing the magnesium aluminum oxide transparent ceramic according to claim 2, wherein the dopamine agent is prepared by dispersing carbon nanotubes into a Tris buffer solution with ph of 9.0 according to a weight ratio of 2.
5. The method for preparing the magnesium aluminum oxide transparent ceramic as claimed in claim 2, wherein the mass fraction of the sodium alginate solution is 10-20%.
6. The method for preparing the magnesium aluminum oxide transparent ceramic according to claim 4, wherein the carbon nanotubes are multi-walled carbon nanotubes with a particle size of 10-20nm.
7. The method for preparing the magnesia-alumina transparent ceramic according to claim 1, wherein the modification method of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into an ethanol solvent which is 5 to 10 times of the total weight of the hydroxyapatite, then adding a silane coupling agent which is 2 to 5 percent of the total weight of the hydroxyapatite and acetaminophen which is 1 to 3 percent of the total weight of the hydroxyapatite, fully stirring, finally washing and drying to obtain the modified hydroxyapatite.
8. The method for preparing the magnesium aluminum oxide transparent ceramic according to claim 7, wherein the silane coupling agent is KH560.
9. The method for preparing the magnesium aluminum oxide transparent ceramic according to claim 1, wherein the chitosan compound lanthanum oxide solution comprises the following raw materials in parts by weight: 4-8 parts of chitosan, 1-3 parts of lanthanum oxide and 20-30 parts of 45-55% sulfuric acid solution by mass fraction.
10. The method for preparing magnesia-alumina transparent ceramics according to claim 1, wherein the operation steps of the temperature-raising heat-improving treatment are as follows: heating to 1300-1320 deg.C at 1-3 deg.C/s, maintaining for 5-10min, and cooling to room temperature with 3-5 deg.C water.
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